Affiliations: Institut für Anorganische Chemie der Universität, Talstrasse 35, D-04103 Leipzig, Germany
Note: [] Corresponding author.
Abstract: The reaction of Li{2,6-(NEt2CH2)2C6H3} with BCl3·Et2O in hexane yields BCl2[2-{BCl3(NEt2CH2)}-6-(NEt2CH2)}C6H3] (1) as the thermodynamically favoured product. If BCl3 · Pyridine is employed, only Cl{2,6-(NEt2CH2)2C6H3} is formed. 1 reacts with [PPh4]Cl to give the BCl3-free product BCl2{2,6-(NEt2CH2)2C6H3} (2) with formation of [PPh4][BCl4]. Li{2-(NMe2CH2)C6H4} reacts with BCl3, to give BCl2{2-(NMe2CH2)C6H4} (3). 1–3 were characterized spectroscopically (NMR, IR, MS) and their crystal structures were determined: 1, T = 260(2) K, triclinic, PT, with a = 7.069(2) Å, b = 10.837(5) Å, c = 14.090(5) Å, α = 90.09(2)°, β = 104.16(2)°, γ = 97.35(2)°, V = 1037.3(7) Å3, Z = 2, d(ca1cd) = 1.429 g cm−3, 3409 independent reflections, and R1= 0.0460, wR2 = 0.0889 (for reflections with I > 2σ(I)), R1 = 0.0752, wR2 = 0.1082 (all data); 2, T = 213(2) K, monoclinic, P21/c, with a = 13.1797(9) Å, b = 7.5833(5) Å, c = 18.6796(13) Å, β = 108.974(1)°, V = 1765.5(2) Å3, Z = 4, d(ca1cd) = 1.238 g cm−3,3174 independent reflections, and R1= 0.0334, wR2 = 0.0824 (for reflections with I > 2σ(I)), R1,= 0.0436, wR2 = 0.0874 (all data); 3, T = 213(2) K, orthohombic, P212121, with a = 9.4540(8) Å, b = 9.5650(8) Å, c = 11.6900(10) Å, V = 1057.1(2) Å3, Z = 4, d(ca1cd) = 1.357 g cm−3, 1913 independent reflections, and R1 = 0.0298, wR2 = 0.0651 (for reflections with I > 2σ(I)), R1 = 0.0334, wR2 = 0.0673 (all data).
